Mineral-oil derivatives



H. T. MAITLAND.

MINERAL OIL DERIVATIVE. APPLICATION FILED JAN. 26, 1921.

1 ,425,885. Patented Aug. 15, 1922.

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HAROLD T. MAITLAND, 0F SHARON HILL, PENNSYLVANIA, ASSIGNOR '10 SUN COM- PANY, OF PHILADELPHIA, PENNSYLVANIA, A CORPORATION OF NEW JERSEY.

MINERAL-OIL DERIVATIVES.

Application filed January 26, 1921.

from mineral oil a saponifiable product and.

a saponified product having the principal qualitiesof animal and vegetable-oils and soaps made therefrom.

My products are derived from materials which are by-products in the manufacture of lubricating oils and other standard refined products from crude oils, which by-products have hitherto either been wasted or only partially utilized for the manufacture of products which command a relatively small price.

This application is a division of an application filed April 15, 1919, Serial No. 290,229. The -process herein described for making my new products is not herein claimed, as it forms the subject-matter of a separate application filed April 15, 1919,

Serial No. 290,228.

In the accompanying drawing, the figure is a vertical sectional view of a mechanical masticator and, digester which I prefer to us in carrying out the process.

lVhile any crude petroleum is possibly or probably adapted for use in the execution of my process, I prefer to use Texas crude oil, or a crude petroleum of that nature on account of the particular group of hydrocarbons and their mobility to conversion which are found in an oil of this kind. The yield is prob-ably increased by the particular distilling process which I preferably employ to secure the so-called lubricating oil stock from which both lubricating oil and my new products are made, and I shall therefore briefly describe such distilling process; although it will be understood that the essential steps of my process may be practiced starting with any lubricating oil stock or distillate, or at least any lubricating oil stock or distillate made by distilling crude petroleum of the proper grade in the ordinary way.

'I first take the crude petroleum and sub- Specification of Letters Patent. Patented A 15, 1922 Serial No. 439,948.

ect it to a preliminary distillation in which all of the crude product is distilled off except a relatively small percentage of residuum. The distillates are then subjected to a second distillation, the heavier product rema nlng in the still being the stock from which lubricating oil may be made. The second distillate is then redistilled, light 011s being distilled off, the part remaining also being adapted for use as lubricating stock.

The lubricating stock is then treated with a mineral acid, preferably sulfuric acid,

with agitation, followed by settlement,

formin a slud e in the bottom of the agitator. f sulfuric acid be used, it should not be the anhydride, or even fuming acid, as otherwise sulfo or other sulphonic acids will be formed, which may be diflicult or impossible to eliminate, or which may make impossible the production of the water-insoluble organic acid product vwhich, when saponied, produces the soap constituting my present invention.

Strictly speaking, the sludge above specified comprises two layers. The lower layer, consisting of a small amount of sulfuric acid, with some sludge in solution, is drawn off and concentrated. The process involves the special treatment of the middle layer, which contains about thirty per cent sulfuric acid and sulphur dioxide. I subject the same to the concurrent action of hot water and mechanical mastication. The Water should be maintained below the,boiling point, during the major part of the process, although it may, i desired, exceed the boiling point until several separations equipped with a steam jacket a bui t to withstand a pressure of one hundred pounds to the square inch. The inside of the digester as well as the movable parts contained within it are covered with some acid-resist ing metal or composition. Special mast cating and stirring paddles b with a certam sweep or pitch are arranged to revolve with a lifting and opposing effect, while stationvertical shaft (Z which moves in an opposite direction to the hollow shaft 6 containing it.

The edges of this paddle which, in rotation, are at the rear, are provided with small openings g, through which water, air or steam, or a mixture of two or all of these, may be introduced into the bottom of the digester by means of the hollow shaft The bottom of the digester is so constructed that large quantities of water, air or steam, or a mixture of them, may be introduced by means of an auxiliary pipe or pipes it. The annular space between the two shafts is flushed with steam or water, entering at 2', so that corrosive chemicals do not come in contact with the unprotected surfaces. Before the sludge is introduced, the digesteris partially filled with cold water at a temperature of approximately 20 degrees C. The desired temperature is maintained through out the operation by means of the steam jacket and live steam blows into the contents through pipes al and h. The introduction of the washing liquid may be intermittent, but is preferably continuous, the surplus liquid passing upward through the sludge and out through an overflow k, carrying with it the undeslrable mineral acid and certain other compounds which may be subsequently treated but the treatment of which forms no part of the present invention. The driving mechanism is so adjusted that the velocity of the masticators or paddles may be diminished or increased at will. The temperature of the contents and the velocity of the masticators are governed entirely by the condition of the sludge as the operation proceeds. The sludge is tested for mineral acidity at certain intervals and when the mineral acid content has been reduced to such an extent say to approximately two per cent) as to give no trouble in the manufacture of the products desired from the sludge, the washing is stopped and the excess washing liquid is syphoned or drawn ofit. During the first part of the operation it is important that no air be permitted to be mixed with the sludge, as the buoyant air with the sulfur dioxide causes the small particles of sludge to rise to the surface and to be carried away with the washing liquid. The residual compounds settling to the bottom of the digester are saponifiable oils containing some. dissolved or suspended minasses eral oil. The product stifi'ens or solidifies on cooling, is. water-insoluble, is practically odorless, does not become rancid; and may be readily saponified with caustic soda or making an ideal road oil or dust preventahe saponified product is partially tive.

soluble in mineral oil, the degree of its solubility depending upon the character of the oil. When mixed with mineral oil and water, it forms a homogeneous emulsion. The sulfur content is about 0.4 per cent, although thiswilfvary somewhat with the degree of thoroughness, or duration, of the continuous washing with hot water. The sulfur probably exists as sulfuric acid or sulfates whose complete removal has not been efi'ected.

Having now fully described my invention, what I claim and desire to protect by Letters Patent is:--

1. As a new product, the herein described derivative from mineral oil, the same being water-insoluble, solid at ordinary temperatures, practically odorless, which doesnot become rancid, and containing a relatively small percentage of sulfur less than about one per cent; the same also being readily saponifiable' and when saponified being soluble in all proportions with water and partially soluble in mineral oil and adapted to undergo the character of hydrolytic decomposition that occurs with soaps derived from animal and vegetable oil.

2. As a new product, the herein described saponified derivative from mineral oil,.. the same being miscible in all proportions with water, partially soluble in mineral oil, containing a relatively small percentage of sulfur less than one per cent, adapted to undergo the character of hydrolytic decomposition that occurs with soaps derived from animal or vegetable oil, and when dissolved in water partially hydrolyzing and after substantially drying not readily dissoluble in water a second time.

In testimony of which invention, I have hereuntosetmyhand, at Philadelphia, Pa. on this 17th day of January, 1921.

HAROLD T. MAITLAND 

